Synthesis and characterization of divalent lanthanide selenolates and tellurolates. X-ray crystal structures of Yb[SeSi(SiMe[sub 3])[sub 3]][sub 2](TMEDA)[sub 2] and (Eu[TeSi(SiMe[sub 3])[sub 3]][sub 2](DMPE)[sub 2])[sub 2]([mu]-DMPE)

Journal Article · Wed Apr 27 00:00:00 EDT 1994 · Inorganic Chemistry; (United States)

DOI:https://doi.org/10.1021/ic00087a012· OSTI ID:6835872

Cary, D R; Arnold, J ^[1]

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1. Univ. of California, Berkeley, CA (United States)

A series of divalent lanthanide chalcogenolates of empirical formula Ln[ESi(SiMe[sub 3])][sub 2](TMEDA)[sub 2] (Ln = Yb, Eu, Sm; E = Se, Te; TMEDA = Me[sub 2]NCH[sub 2]CH[sub 2]NMe[sub 2]) and (Eu[ESi(SiMe[sub 3])[sub 3]][sub 2](DMPE)[sub 2])[sub 2]([mu]-DMPE) (E = Se, Te; DMPE = Me[sub 2]PCH[sub 2]CH[sub 2]PMe[sub 2]) have been prepared by the reaction of Ln[N(SiMe[sub 3])[sub 2]][sub 2](THF)[sub 2] (Ln = Yb, Eu, Sm) with HESi(SiMe[sub 3])[sub 3] (E = Se, Te) in diethyl ether with excess TMEDA or DMPE. Both Yb[SeSi(SiMe[sub 3])[sub 3]][sub 2](TMEDA)[sub 2] and (Eu[TeSi(SiMe[sub 3])[sub 3]][sub 2](DMPE)[sub 2])[sub 2]([mu]-DMPE) have been structurally characterized by X-ray crystallography. Yb[SeSi(SiMe[sub 3])[sub 3]][sub 2](TMEDA)[sub 2] crystallizes at -40 [degrees]C from hexanes in the space group P2[sub 1]/c with a = 9.441(2) [angstrom], b = 12.311(2) [angstrom], c = 23.407(7) [angstrom], [beta] = 96.013(21)[degrees], V = 2705.4(11) [angstrom][sup 3], d[sub calcd] = 1.30 g cm[sup [minus]3], and Z = 2. (Eu[ESi(SiMe[sub 3])[sub 3]][sub 2](DMPE)[sub 2])[sub 2]([mu]-DMPE) crystallizes at -40 [degrees]C from hexanes in the space group P[bar 1] with a = 13.629(2) [angstrom], b = 13.696(2) [angstrom], c = 17.642(3) [angstrom], [alpha] = 81.715(13)[degrees], [beta] = 78.828(12)[degrees], [gamma] = 89.452(13)[degrees], V = 3190.2(12) [angstrom][sup 3], d[sub calcd] = 1.33 g cm[sup [minus]3], and Z = 2. On being heated to ca. 200 [degrees]C in the solid state, the Yb-TMEDA compounds eliminate E[Si(SiMe[sub 3])[sub 3]][sub 2] to form the corresponding divalent chalcogenides as dark, microcrystalline powders.

• OSTI ID: 6835872
• Journal Information: Inorganic Chemistry; (United States), Journal Name: Inorganic Chemistry; (United States) Vol. 33:9; ISSN 0020-1669; ISSN INOCAJ
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
400201* -- Chemical & Physicochemical Properties
CHEMICAL PREPARATION
COHERENT SCATTERING
CRYSTAL STRUCTURE
DIFFRACTION
EUROPIUM COMPOUNDS
LATTICE PARAMETERS
ORGANIC COMPOUNDS
ORGANIC SILICON COMPOUNDS
RARE EARTH COMPOUNDS
SCATTERING
SELENIUM COMPOUNDS
SYNTHESIS
X-RAY DIFFRACTION
YTTERBIUM COMPOUNDS